Hydrogenation and dephlegmation apparatus



Feb. 27, 1934.- M, J. TRUMBLE Er AL HYDROGENATION AND DEPHLEGMATION APPARATUS Filed Deo. 13, 1950 INI/ENTORS .7. TRU/v5.45

/I TTORNE YS.

Patented Feb. 27, 1934 HYDROGENATION AND DEPHLEGMATION APPARATUS Milon J. Trumble, Alhambra, and william L. Seeley, Los Angeles, Calif., assgnors to Processco, Limited, San Francisco, Calif., a co1'- poration of Nevada Application December 13, 1930 Serial No. 502,145

7 Claims.

This invention relates to the manufacture of gasoline from heavier hydrocarbon oils as by cra/cking, hydrogenation, or both, particularly to a process for which a copending patent application has been led by us simultaneously herewith under Serial No. 502,146, and entitled Hydrogenation process and apparatus.

The principal object of our invention is to provide a preferred construction for one of the apparatus units to be used in carrying out the process of the aforesaid application in dephlegmating and hydrogenating vapors and oil at certain stages of said process, particularly at the points D, M and T designated on the flow sheet of said process being Fig. 1 of the drawing of said application.

Another object is to provide a more efcient method of dephlegmation and hydrogenation by combining the same, still another object is the provision of apparatus which may be used to advantage in almost any cracking or hydrogenating plant for separating of the reflux oil and hydrogenating the vapors. Other objects will appear in the following description and accompanying drawing.

In the drawing Fig. 1 is a vertical section of one form of our apparatus.

Fig. 2 is a cross section of the apparatus as seen from the line 2-2 of Fig. 1.

Fig. 3 is a cross section as seen from the line 3-3 of Fig. 1.

Fig. 4 is a cross section as seen from the line 4 4 of Fig. 1.

Fig. 5 is a cross section `as seen from the line 5 5 of Fig. 1.

Before describing the apparatus `in detail it might be mentioned that some of the designating characters are the same as used on the ow sheet Fig. 1 of the copending case referred to so that its relation thereto will be easily established. These characters are D, Z', 5,52, 53 and 55.

In further detail the apparatus comprises a cylinder D suitably mounted upright on a base 1 and in localities where necessary is suitably heatinsulated as indicated for a portion of the cylinder at 2.

` The cylinder is best made in sections bolted together by nange joints as at 3 so that it may easily be assembled or disassembled.

Within the cylinder s a series of spaced horizontally arranged disks or plates 4 each provided with a relatively large central opening surrounded with a downwardly extending collar 6 projecting at its lower end through a somewhat larger opening in an inwardly curved deflector 7 in turn supported at its lower edge from a downwardly turned or inverted cup-like member 8 in turn supported centrally in a ring-like screen plate 9 in turn supported at its marginal edge by small angles l() secured to the inner wall of the cylinder.

Member 7 is perforated with a few small holes at 11 where it joins member 8 for return flow of reflux oil removed from ascending vapors, but members 4 are preferably imperforate, and under each is a steam coil 12 connected to a separate source of steam 52 and each provided with a valve as at 56 for separate control.

The screen disks or rings 9 are for the purpose of carrying each a layer of catalytic material such as nickel oxide which may be renewed from time to time through hand holes covered with removable plates 13.

The lowermost plate 4 isspaced above the lower end of the cylinder to provide room for entering vapors and gases from a pipe 5 and a settling chamber for reflux oil 14 which is led off through a pipe for forcing by means of a pump Z1, to further treatment or to storage, a suitable cat controlled automatic pump feed tank 15 of any conventional design being interposed between the pump and cylinder to prevent access of gas to the pump and starting the same when sufficient liquid is present.

Spaced above the uppermost of the inverted cups 8 is a circular condensation pan or reservoir 16 which is suspended from the underside of a transverse wall 17 which together with a similar wall 18 forms a heat exchange space 19 surrounding a battery of small vertically arranged cooling tubes 20 passing through and tightly welded or brazed at their ends to plates 17 and 18, while the head of the cylinder is spaced above the upper end of the cooler assemblage and provided with a vapor take-off pipe 53 through which the dephlegmated vapors pass for 9 condensation to gasoline in any desired form 0i' condenser.

The upper edge of condensation pan 16 is spaced a short distance below the lower end oi' the cooling tube assemblage both for the upward passage of gases and vapors from the cylinder through the tubes, as well as for marginal overflow of reflux oil for dribbling back through the screens and over the shelf-like arrangement of plates to the oil compartment at the bottom of the cylinder.

A pipe 21 is also provided for the purpose of by-passing reilux oil from pan 16 to the lower end of the cylinder and provided with a valve at 22.

Heat exchange space 19 is provided with inlet and outlet pipes 23, 24 for the circulation of any oil or other fluid which it is desired to heat at some stage of the processes in which the apparatus is used.

In operation the hydrocarbon vapors of the cracking or hydrogenating still together with free hydrogen or mixture of hydrogenating gases such as disclosed in our copending case enter from pipe 5 for circuitous passage upward as indicated by the arrows. The hydrogen is trapped, or that is, accumulates in each inverted cup 3, and the vapors pass out over the lower edge of the cup carrying hydrogen with them and up through the screens of catalytic material, then laterally over the steam coils, then downwardly through the annular space atthe inner edge of deflectors 7 and upwardly into the next hydrogen cup etc.

The coils 12 are supplied with steam at various temperatures, and are generally adjusted to give sharp drops in temperature of about 100 F. each starting with about 900 F. for the lowermost one, assuming the gaseous mixture to be treated to be entering at about 1000 F., and terminating with about 500 F. with the upper coil and additional lowering of temperature in the cooling tubes to about 400 F, the vapors -being automatically maintained at a constant pressure of about 100 pounds per square inch by suitable pressure control apparatus not shown.

As the apparatus is heating up, the reux oil is run through by-pass pipe 21 but after the temperatures of the various zones are secured the pipe is shut oi so that the reflux oil returns counterflow to the ascending gases. Thus the gases are successively passed over coils of various temperatures with alternate submission to the action of hydrogen in the inverted cups and the inuence of the catalyst carried on the screens, while the returning oil from above meets the same steps of temperature in reverse order, so that the various fractions are submitted to vapor phase hydrogenation at a' plurality of temperatures so as to present each at a temperature suitable for its reaction, and the returning oil is resubmitted to these various temperatures for liquid phase hydrogenation.

Through the construction provided it is manifest that there may be any number of steam coils, traps and screens, and that some of the coils may be supplied with wet steam or other cooling uids instead of superheated steam, so that the ascending vapors will be subject to alternate chilling and heating to hydrogenate some of the unsaturates which hydrogenate at lower temperatures than the partial saturates, such for instance asbenzol which hydrogenates best at a temperature of about 409 F. The approximate reaction at this temperature being C6H6-l-3H2=C6H12l39,300 calories and this reaction is carried still further in an excess of hydrogen in the presence of the catalyst until another molecule of H2 is added to form 06H14, a complete saturate of the gasoline series, though if reverse action is desired, that is, more benzol or anti-knock properties, the temperature may be raised to nearly 1100 F. where the formation of the benzol series is favored.

The reflux oil which falls to the lower end of the hydrogenator-dephlegmator and continually carried away by pump Z1, is in the complete process of our copending case above mentioned converted to vapor and treated to vapor phase hydrogenation, but in some cases it may be recycled through the steps of the process of which it is the product, or it may be run to storage.

We claim:-

1. Petroleum hydrogenating and dephlegmating apparatus comprising an elongated upright cylindrical container, means for admitting petroleum vapors into the lower part of the cylinder and passage out of the top of the cylinder, a plurality of spaced shelves across said cylinder each with an opening for upward passage of vapors, a heating coil under each shelf, screens extending across the cylinder spaced intermediate said shelves, inverted vapor-retaining cups at each screen positioned over the opening in a shelf, and means for separately controlling the temperature of each heating coil.

2. Petroleum hydrogenating and dephlegmating apparatus comprising an elongated upright cylindrical container, means for admitting petroleum vapors into the lower part of the cylinder and passage out of the top of the cylinder, a plurality of spaced shelves across said cylinder each with an opening for upward passage of vapors, a heating coil under each shelf, screens extending across the cylinder spaced intermediate said shelves, inverted vapor-retaining cups at each screen positioned over the opening in a shelf, deflectors below each heating coil arranged to deiiect the ascending vapors against the coil and into the opening of the shelf above, and means for separately controlling the temperature of each heating coil.

3. In a construction as specified in claim 2, drainage means controlling counterow of condensate through a limited area of said screens.

4. Petroleum hydrogenating and dephlegmating apparatus comprising an elongated upright cylindrical container, means for admitting petroleum vapors into the lower part of the cylinder and passage out of the top of the cylinder, a plurality of spaced shelves across said cylinder each with an opening for upward passage of vapors, a heating coil under each shelf, screens extending across the cylinder spaced intermediate said shelves, inverted vapor-retaining cups at each screen positioned over the opening in a shelf, deflectors below each heating coil arranged to deflect the ascending vapors against the coil and into the opening of the shelf above, and means for separately controlling the temperature of each heating coil, said deflectors provided with drainage opening guiding condensate to drip through a limited area of said screens.

5. Petroleum hydrogenating and dephlegmating apparatus comprising an elongated upright cylindrical container, means for admitting petroleum vapors into the lower part of the cylinder and passage out of the top of the cylinder, a plurality of spaced shelves across said cylinder each with an opening for upward passage of vapors,

a heating coil under each shelf, screens extendthe opening or the shelf above, means for separately controlling the temperature of each heating coil, said deectors provided with drainage opening guiding condensate to drip through a limited area of said screens, and a valved pipe for optionally passing condensate from the upper part of the cylinder past said shelves and screens to the bottom of the cylinder.

6. In a construction as specified in claim 1, a collar extending downwardly around each shelf 

